Krzek Jan, Starek Malgorzała
Department of Inorganic and Analytical Chemistry, Collegium Medicum, Jagiellonian University, 9 Medyczna Str., 30-688 Cracow, Poland.
J Pharm Biomed Anal. 2002 Apr 15;28(2):227-43. doi: 10.1016/s0731-7085(01)00622-7.
A chromatographic-densitometric method for identification and quantitation of diclofenac and its impurities, i.e. 1-(2,6-dichlorophenyl)indolin-2-one and indolin-2-one in pharmaceutical preparations and model solutions was developed. The effect of pH, temperature and ultra violet (UV) radiation on diclofenac's concentration was investigated. Chromatographic separation was performed on TLC silica gel coated plates with the mobile phase: cyclohexane-chloroform-methanol (12:6:1, v/v/v). Densitometric detection was carried out in UV at lambda=248 nm. The conditions for good separation and the detection limit were established. The recovery for diclofenac was 99.20%, for 1-(2,6-dichlorophenyl)indolin-2-one--92.34% and for indolin-2-one--95.85%. The method was used for quality assessment of diclofenac in pharmaceutical preparations. Reliable results comparable to those determined by high performance liquid chromatography (HPLC) were obtained.
建立了一种用于鉴定和定量药物制剂及模型溶液中双氯芬酸及其杂质（即1-(2,6-二氯苯基)吲哚啉-2-酮和吲哚啉-2-酮）的色谱-密度测定法。研究了pH、温度和紫外线（UV）辐射对双氯芬酸浓度的影响。采用环己烷-氯仿-甲醇（12:6:1，v/v/v）作为流动相，在硅胶薄层板上进行色谱分离。在波长λ=248nm的紫外光下进行密度测定检测。确定了良好分离的条件和检测限。双氯芬酸的回收率为99.20%，1-(2,6-二氯苯基)吲哚啉-2-酮为92.34%，吲哚啉-2-酮为95.85%。该方法用于药物制剂中双氯芬酸的质量评估。获得了与高效液相色谱（HPLC）测定结果相当的可靠结果。
